Solidified oil and process of making same.



o the pine riyed'.

' deeto the and similar material and the is mixed with soap solutions,

put pine oil and similar oils into a UNITED STATES rATEuT orricn.

CABLET ON ELLIS, OF MONTCLAIR, NEW JERSEY, ASSIGNOR TO ELLIS-FOSTERCOMPANY, A CORPORATION OF NEW JERSEY.

SOLIDIFIED OIL AND PROCESS OF MAKING SAME.

1,109,119. No Drawing.

Speciflcation of Letters Patent. Application flledliarch 29, 1910.Serial No. 552,177.

Patented Sept. 1, 1914.

To all whom it may concern Be it known that I, CARLETON ELLIS, a citizenof the United States, residing at Montclair, in the county of Essex andState of New Jersey, have invented certain new and useful Improvementsin Solidified Oils and Processes of Making Same, of which the followingis a specification.

T hisinvention relates to solidified oil compositions and to the processof making same and relates particularly to the solidified pine oilsmadefrom long leaf pine oil products solid product derived from cresylicacid and similar carbolic acid material. Ordinary pine oil, for example,is, a liquid insoluble'in water and having no power of itself of readilyemulsifying with water. If however, the pine oil emulsions may beobtained. By the use of concentrated soaps, such as oleate of potash,the pine oil becomes more or less miscible with water and certainpreparations known as soluble pine oils which are of this character arenow on the market.

The objeect of the present invention is to solid form and particularlyinto a form in which they are only slightly soluble in water, but whichby the action of water, become slowly soluble or miscible thus becomingcapable of distributing themselves in fine particles throughout .a largebody of water. The ordinary long leaf pine oil may be solidified by theincorporation with it of stearic acid and subsequent addition of causticsoda, to produce a soap in a concentrated condition. In the absence ofmore than a very small amount of water, practically that amount whichjust sufiices to put the caustic soda in solution, and at an elevatedtemperature, oil dissolves the sodium stearate, and on cooling.solidifies to a hard solid materiali 0n the other hand if oleic acid isused with caustic potash, for example, as the saponifying agent, aliquid material is de- This is usually of a dark grown color use of redoil or commercial oleic acid, while the stearic acid products areusuallywhite and even transparent if the proportion of stearic acid soap is nottoo great and if the temperature has been tained however if As anillustration to 14 pounds of, pinc Oil and 1 pound of stearic acidcommingled ao and incorporated by heat,'wlien thestearic acid hasthoroughly dissolved in the pine 01], 35 pound caustic soda dissolved inslightly more than its own weight of water is added and the mixturestirred thoroughly, the heating being carried up preferably nearly tothe boiling point of the pine oil in order to secure properincorporation. At temperatures of for example, 40 or 50 C., a sort ofcoagulation occurs and a very unsatisfactory product results. If thetemperature is carried to say 100 C., the. product is usually firm andsomewhat opaque. If however the temperature is carridilip to nearly theboiling point of the transparent material may e produced. It isdesirable however in actual practice to use steam jacketed kettles formanufacturing the product and for that reason, a temperature of 100 to135 C. is perhaps more-feast. ble. It 1s alsodesirable, after thematerial has been incorporated, to chill the product so as to preventsegregation which often occurs on slow cooling. This is very readilydone in a jacketed kettle by substituting cold water in the jacket forthe steam previously used for heating. The product 0bdesired may be castin molds which preferably should be chilled, and also preferably shouldbe exposed a short time to the air or to a vacuum before shipment, inorder to develop a high degree of firmness which such air or vacuumexposure tends to bring about. The pine oil product made in this manneris fairly soluble. If a small block of material is placed under runningwater, it may dissolve in'from 20 to 30 minutes. For'some purposes, sucha high grade of solubility is undesirable and to reduce the solubility,I incorporate with the pine oil, for certain purposes, various oilssuclt as refined mineral oils or crude petroleum. For example, in theabove formula, if crude petroleum is substituted for one-thirdor'one-halfv inasmuch as large cakes of the material may I 4 t v I me'Oll, a clear v be placed in the water and as these slowly I glvespecial odors or u ber dlssolve, the pine oil and crude petroleum oilspread. over the surface of the water, the insectifugal odors of thepine oil driving the mosquitoes from the neighborhood and the crudepetroleum oil effectually sealing the surface of the water so as toprevent reproduction of the mosquitos. Of course, various mineral oilsmay be used instead of crude petroleum oil and an oil of about .865specific gravity derived from petroleum, is a very useful material forthis purpose. Waxes act in a somewhat similar manner as respectsreduction of solubility but are more expensive and are therefore morelimited in application. Crude paraffin wax including scale wax and thelike are however fairly cheap and may be included in varying amounts tosecure various degrees of solubility. For example, in the formula abovementioned, the incorporation of 25% of scale wax reduces the solubilityof the material and 50% makes the product very hard and slightlysoluble; with the addition of 75%, the material becomes practically tooinsoluble to be of any great value for most applications. On the otherhand, with the addition of 50% to 75% mineral oil, very oily solidproducts may be secured which have certain very desirable properties. Inlieu of waxes, naphthalene may be employed to a greater or less extent.For example, in the above formula comprising pine oil, stearic acid andcaustic soda, 5%, 10% and upward to say 40 or 50% of naphthalene may beincorporated. With the lower percentages, very little crystallization isevident on. cooling, but with the larger percentages, crystallization isso much in evidence that the masses oftentimes are somewhat crumblyespecially after water has acted upon the material for a short time.These solidified oils may be given various colors by the use of oilsoluble dyes. They maybe combined if desired with filling or weightingmaterials as for example, if

cake heavier than water, such substances as talc, infusorial earth, oxidof iron, etc., may. be em loyed, while, if it is desired to have thecaiie lighter than water, such materials as sawdust, wood flour,-starch', sugar and the,

like may be made use of. Also other essential oils'may be included if itis desired to .special medicinal or product. Of course, w, t degra woolgrease, lanolin ,.various resins such as colophony, dammar, ianak,guayule and similar. resins, may be incorporated to a greater or lessextent in accordance with the character-of the product desired forspecial applications.

other properties to the h d guayule'gums' containing both-the andresinous material. Metallic and for similar it is desired to have the.

I additional dar e. coral, .P nti-' Also rub: oducts particularly thecrude Pontisoaps such as aluminum palmitate, zinc stearate and the likemay be added as desired. I

In the solidification of creosote, toproduce a solidcomposition forpreparing shee purposes, the formula may be varied as followszcresylicacid'10 pounds, stearic acigl, 1 poufdfca ustic soda 1- of a poii'lidiThis gives a product of mod: erate solubility which may be rendered moresoluble by the incorporation of potassium oleate or sulfonated oils.Similarly with the pine oil, should it be desired to secure anespecially soluble product, sulfonatedoil in its concentrated liquid orsolid forms, or potassium oleate or any similar soap material, may beintroduced to advantage, care being taken to not use such proportions asto cause liquefaction.

The process may be applied to various oilssuch as oil of cedar, oil ofcedar leaf, oil of camphor, oil of lemongrass and oils of birch tar,cajeput, mace. nutmeg and the like to secure a solid product. In orderto produce a clear product it is desirable to heat the oil afterincorporation of the soap to a temperature above the boiling point ofwater, until the water is eliminated, care being taken to agitate theoil well during this process as the boiling is oftentimes violent. Ifalcohol is used instead of water as the tion may take This is especiallythe case with methyl alcohol which boils at 66 C. In the case of certainessential oils which have rather low boiling points and which jection tohigh temperatures, the use of an alcoholic solvent is to be recommended.

In case of cresylic acid or other carbolic acid materials, thesolidification may be made such that the product may be cut out into theshape of tablets for medicinal uses are injured by suband may be made sofirm as to be capable of supporting a coating of some other material.The addition of a little more alkali than that actually required for thecombination with the fatty acid employed is usually desirable in thesolidification of cresylic acid material. In the case of pine oil aswill appear from the foregoing formula, 25% of caustic soda has beenused reckoned on the amount of stearic acid, while the actualSaponification requires onl about 20%.- This uantity of kali ishowevennot obiectionab e andis rather desirable in or: der to rapidlycomplete saponification. The material may however be made substantiallyneutral by using the exact equivalent of alkali. The stearic acid may bereplaced by still stockto advantage in some cases.

The present invention therefore involves the process of melting orincorporatin the essential oils" to be solidified, with eelysaponifiable soap-forming fatty acids, adding as caustic soda, carbonateof soda, potashor whatever the alkali maybe, preferably just sufficientwater the alkali in-solut-ion, combini'n fthis, preferably hot, withtheoil, prefera ly hot, carrying the freely s aponifiable fatty acid-andagitating'to effect perfect incorporation and substantial solution ofthe soap, referably followed by the step of heating t e oil to atemperature suflicient to expel a substantial portion or all of thewater whereupon the mass preferably is rapidly chilled to insure propersetting andto overcome segregation. in -It will b evident tothoseskilled in the art, from the information herein set forth, that variousmodificationsmay be made under the present invention to produce bodiesof different proportions and suited for many '20 difierent'applications,and I do not wish to limit; myself strictly to the invention; as hereinset forth and wish. to'qapply or invoke the doctrine same may be hereinapplicable, all in view of the present State, of the art and'with duerecognition" of the heretofore employed methods or. making soluble orsolidified oils in various ways, by the use in'some cases of dissolvedin soaps either to produce emulsions or miscible v 50 oils in a mannerforeign to the idea of the present invention, but in some cases employi'ng'materials more orless similar in charac: ter to produce bodieshaving different properties or characteristics from those herein asdescribed. The products made under my invention are characterized bytheir peculiar.

colloidal condition manifestmg itself 1n va rious ways. Some of thecompositions here'- under for example are readily fusible when 40 firstformed but become difiicultlyfusible on standing. Seemingly the soap,forming as it does in the oil itself exerts by nascent action somepeculiar colloiding influence on the oil and it is probably because ofthis condition of nascency thatfirmer, sounder prod- -Especially doesthis seem ucts are obtained. a morepotendfactor after reaction is welltov maintain of equivalency so far as under way the mass is quicklychilled, therey molecular soap complexes.

' By pine oil, orpilof pine,

possibly preventing the formation of as used herein, "j Ireferparticularly to the'volatile oils derived from genus Pinus and morespecifically refer to spirits of turpentine, Russian turpentine, andlong leaf pine oil.

v.I claim:-

' I 1. The herein described firm solid insectifugal compositioncomprising an essential oil' and a modicum of a soap of stearic acidwith sufiicient additional water -'insoluble material to substantiallyreduce the solubility ofthe solidified product in water, saidcomposition being prepared at a temperature above 190 0. whereby itbecomes clear and transparent.

2.,The herein de'scribed'firm, solid insectifugal composition comprisingan essential oil and a modicum of a sodium soap 'of' stearic acid withsuficient additional waterinsoluble material the solubility of thesolidified product in water, said composition being prepared" at atemperature above 100 C. whereby it be comes clear and trans arent;

3. The herein descr bed solid insectlfugal composition comprising pineoil, naphtha-' lene anda modicum or sodium stearate so to substantiallyreduceblended as to constitutea clear and trans-.51

parent mass.

4. The herein composition comprising'pine oil, naphthalene'and ,amodicum o 'sodiumstearate incorporated with a non-volatile 'oil .to substantially reduce the solubility of the solidified product in water; thecomponents of said composition being so blended as to constitute a'clearand transparent cake;

-In testimony whereof I have aflixed my signature 1n presence of twowitnesses.

a oABLE'rON. nLLis.

Witnesses:

NATHANIEL L. Eos'rER, J AMES EMon'r.

described solid insectifu gal-

